CN111018536A - Carbon-ceramic composite material heater and preparation method thereof - Google Patents

Carbon-ceramic composite material heater and preparation method thereof Download PDF

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CN111018536A
CN111018536A CN201911302476.XA CN201911302476A CN111018536A CN 111018536 A CN111018536 A CN 111018536A CN 201911302476 A CN201911302476 A CN 201911302476A CN 111018536 A CN111018536 A CN 111018536A
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carbon
composite material
ceramic composite
ceramic
heater
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CN111018536B (en
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廖寄乔
石磊
邓华峰
李丙菊
李军
王冰泉
彭信辉
刘学文
王跃军
龚玉良
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KBC Corp Ltd
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Abstract

The invention discloses a preparation method of a carbon-ceramic composite material heater for a single crystal furnace, which is uniform in silicon carbide distribution and low in preparation cost, and comprises the following steps of preparing ceramic slurry from ⑴, preparing a wet blank of the carbon-ceramic composite material heater from ⑵, and preparing carbon-ceramic composite material from ⑶ for heatingThe method realizes the introduction of ceramic powder and a lubricant comprising graphite powder or graphene into a carbon fiber preform in a physical mode at room temperature, and prepares the carbon-ceramic composite material heater after vapor deposition, has the characteristics of simple process, short production period, low preparation cost, good conductivity and the like, can well control the resistivity of the carbon-ceramic composite material by adjusting the ceramic content in the carbon-ceramic composite material, and has the open porosity of 1-9% and the density of 1.5g/cm3～2.3g/㎝3The bending strength is 250 MPa-480 MPa, and the resistivity is 10 mu omega-300 mu omega-m.

Description

Carbon-ceramic composite material heater and preparation method thereof
Technical Field
The invention relates to a single crystal furnace, in particular to a carbon-ceramic composite material heater and a preparation method thereof, and especially relates to a carbon-ceramic composite material heater for a single crystal furnace, which has the advantages of uniform distribution of ceramic powder in a carbon-ceramic composite material and low preparation cost, and a preparation method thereof.
Background
At present, most heaters in the single crystal furnace are in a slotted fence cylindrical shape. In the aspect of structural design, in order to match the resistance, a pair of end-to-end parallel resistance strips are formed by processing axial grooves which are sequentially distributed and only penetrate through the upper end surface or the lower end surface on the cylinder body. In terms of the material used, graphite or carbon-carbon composite materials are mostly adopted. During use, the reaction between the carbon material and the Si-rich atmosphere in the thermal field can change carbon into CO, so that the matrix of the carbon material is eroded continuously. Because the cross section area of the top of the slot arc on the carbon heater cylinder body is smaller and is an inflection point of the shape, namely the current flow direction, the corrosion is most easily caused. Once corrosion begins, the size of the point becomes thinner and thinner due to corrosion, the current density becomes larger and larger, the reaction speed becomes faster and faster, a vicious circle is formed, the product is integrally disconnected after the open groove penetrates to the end face of the heater along the groove top, and the circuit is disconnected and cannot be used. Although carbon heaters have been dedicated to increasing the density of products, particularly carbon-carbon composite heaters, which can produce a very dense carbon coating on their surface, the intrinsic property of reacting with a silicon-rich atmosphere is still not solved, and only the corrosion is delayed. So that the heater becomes the shortest life of all thermal field components, and great cost pressure is brought to the industry.
By studying the reaction mechanism of the carbon material and the silicon-rich atmosphere, it can be found that the carbon material is finally generated into silicon carbide and exists stably. Therefore, we believe that the problem of susceptibility to corrosion of the heater can be fundamentally solved by introducing silicon carbide into the carbon heater so that it provides protection to the entire heater.
Document 1: the invention patent CN 101905977A discloses a preparation method of an integral heater of a carbon/carbon polycrystalline silicon ingot furnace. Winding carbon cloth or a needled carbon felt which is coated with resin on a steel mold core layer by layer to prepare a prefabricated body; the density of the heater product is more than or equal to 1.50 g/cm through pressurization curing, carbonization and chemical vapor deposition densification treatment3(ii) a The shape and the size required by a customer are achieved through machining; and finally, preparing the carbon-carbon composite material polycrystalline silicon ingot furnace integral heater through a CVD silicon carbide protective layer and high-temperature purification treatment. According to the preparation method, the silicon carbide coating is prepared on the surface of the carbon heater, and compared with the existing carbon material heater, the consumption of raw materials is reduced by more than 90%; the CVD surface deposited silicon carbide protective layer on the surface of the product can prevent the product from being corroded by silicon vapor, oxygen and the like, and the service life of the product is prolonged by at least one time.
Document 2: the invention patent CN 103833402A discloses a silicon carbide ceramic composite material inner heater protection tube and a preparation method thereof. The inner heater protection tube made of the silicon carbide ceramic composite material comprises an outer silicon carbide layer, an inner silicon carbide layer and a carbon fiber reinforced layer, wherein the outer silicon carbide layer is arranged on the outer surface of the carbon fiber reinforced layer, and the inner silicon carbide layer is arranged on the inner surface of the carbon fiber reinforced layer. The protection tube of the internal heater made of the silicon carbide ceramic composite material has the advantages of high thermal conductivity, good thermal shock resistance, corrosion resistance and long service life; when the method is used in the field of smelting metals such as zinc, aluminum, silver and the like, the times and the cost of equipment shutdown maintenance and replacement can be reduced, the production efficiency is obviously improved, and the production cost is reduced.
However, the above patents all rely on the difference in thermal expansion coefficient between the silicon carbide and the carbon/carbon matrix, and the heater is subjected to repeated thermal shock, which easily causes the silicon carbide coating to crack and fall off due to the mismatch of thermal expansion coefficients, thereby causing the failure of protection.
At present, a heater for a single crystal furnace is prepared by adopting a carbon ceramic composite material is rarely reported. The preparation method of the carbon-ceramic composite material mainly comprises the following steps: (1) chemical vapor infiltration deposition (CVI), which is a method of depositing gas generated by cracking silicon organic matters at high temperature into the interior of a prefabricated part to form a carbon-ceramic composite material, and has the defects of long preparation period, poor uniformity of a deposited ceramic matrix and high preparation cost; (2) a precursor impregnation pyrolysis process (PIP) is characterized in that polymer silane is used as a precursor to be impregnated into a porous fiber preform, then the polymer silane is pyrolyzed at high temperature to generate a ceramic matrix in situ, and the ceramic matrix is finally treated for multiple times to obtain a carbon-ceramic composite material, wherein the preparation period is long, and the adhesion force of silicon carbide on fibers is poor; (3) the method comprises the steps of melting silicon powder at high temperature, permeating the silicon powder into a carbon fiber preform through capillary action, and reacting the silicon powder with pyrolytic carbon in the carbon preform to generate silicon carbide to finally obtain the carbon-ceramic composite material (RMI). The method is simple, quick and low in cost, but has the defects that silicon carbide particles are large and uneven in distribution, the mechanical property of the whole material is reduced due to the fact that melt silicon reacts with deposited carbon and carbon fibers, and the stability and the high-temperature performance of the carbon-ceramic composite material are affected by redundant silicon.
Disclosure of Invention
The invention aims to provide a carbon-ceramic composite material heater for a single crystal furnace, which has the advantages of uniform distribution of ceramic powder in a carbon-ceramic composite material and low preparation cost, and a preparation method thereof.
The invention adopts the following technical scheme to realize the aim of the invention, and discloses a preparation method of a carbon-ceramic composite material heater, which comprises the following steps:
⑴, preparing ceramic slurry, namely, mixing ceramic powder, a dispersant and a solvent uniformly by stirring and ball milling, adjusting the pH value of the solution, and preparing suspended ceramic slurry, wherein the ceramic slurry also comprises a lubricant, the lubricant is one of graphite powder or graphene, and the mass ratio of the ceramic powder to the lubricant is 1: 0.1-0.3, the pH value of the prepared ceramic slurry is 11.8-12.0, the solid content of the ceramic powder is 10-30%, and the viscosity is 50-200 mPa.S;
in step ⑴, the ceramic powder is one or more of silicon carbide, silicon nitride or boron carbide, the particle size of the ceramic powder is 0.1-10 μm, the purity is 99.0%, the dispersant is one of polyvinyl alcohol, polyethylene glycol, epoxy resin or phenolic resin, the solvent is distilled water, and the mass ratio of the ceramic powder to the dispersant to the solvent is 1: 0.05-0.1: 2.23-8.95.
In step ⑴, the particle size of the graphite powder is 1-10 μm, the purity of the graphite powder is 99%, the particle size of the graphene is 35-50 μm, and the purity of the graphene is 95%.
In step ⑴, the pH value is adjusted by using 30% hydrochloric acid and acrylamide or liquid ammonia as an alkali.
⑵ preparing a wet blank of the carbon ceramic composite heater, namely alternately laminating and needling a carbon fiber mesh tire and carbon fiber cloth into a carbon/carbon preform according to a drawing, needling the carbon/carbon preform by a needling mechanism, wherein the needling mechanism comprises a needle seat, and an injection needle and a needling needle are arranged on the needle seat;
applicants' method in step ⑵, where the carbon fiber cloth isIs a unidirectional cloth or an interwoven cloth with the surface density of 500g/m2～ 1400g/m2(ii) a The areal density of the net tyre is 30g/m2～130g/m2(ii) a The needling depth is 6-25 mm, and the needling density is 4 times/cm28 times/cm2Injection density of 1 times/cm 22 times/cm2(ii) a The number ratio of the injection needles to the acupuncture needles is 1: 4-6, wherein the length of the injection needle is longer than that of the acupuncture needle by 2 +/-0.1 mm.
In step ⑵, the pressure during injection is 0.25MPa to 0.45MPa, and the injection amount of the ceramic slurry is 2.0 g/cm3～4.67g/㎝3The introduction amount of the ceramic powder in the carbon-ceramic composite material heater wet blank is 0.2 g/cm3～1.4g/㎝3。
⑶, preparing a dry blank of the carbon-ceramic composite material heater, namely, putting the wet blank of the carbon-ceramic composite material heater prepared in the step ⑵ into an environment with the temperature of 100-200 ℃ for processing for 6-24 h to prepare the dry blank of the carbon-ceramic composite material heater, wherein the density of the dry blank of the carbon-ceramic composite material heater is 0.6 g/cm3～2.0g/㎝3；
⑷, rough machining, namely rough machining is carried out on the carbon-ceramic composite material heater dry blank according to a drawing, and allowance required by subsequent machining is reserved;
⑸ vapor deposition, namely putting the carbon-ceramic composite material heater dry blank prepared in the step ⑷ into a vapor deposition furnace for vapor deposition;
in step ⑸, during vapor deposition, natural gas or methane or propane is used as a raw material, the deposition pressure is 1 kPa-3 kPa, and the deposition temperature is 950 ℃ -1200 ℃;
⑹, repeating the steps ⑷ and ⑸ to the set deposition density, and carrying out finish machining according to a drawing to manufacture the carbon-ceramic composite material heater, wherein the open porosity of the carbon-ceramic composite material heater is 1-9%, and the density is 1.5g/cm3～2.3g/㎝3The bending strength is 250 MPa-480 MPa, and the resistivity is 10 mu omega-300 mu omega-m.
In order to prevent corrosion and prolong the service life, after the step ⑹, the method carries out a step ⑺, and the carbon-ceramic composite material heater is placed into a silicon carbide CVD furnace for carrying out surface deposition of a SiC coating, wherein the thickness of the coating is 5-2000 mu m.
In step ⑺, during vapor deposition, trichloromethylsilane is used as the raw material, hydrogen is used as the carrier gas, argon is used as the diluent gas, the deposition pressure is 1 kPa-3 kPa, and the deposition temperature is 900 ℃ -1250 ℃.
The carbon-ceramic composite material heater prepared by the method is characterized in that the open porosity of the heater is 1-9%, and the density is 1.5g/cm3～2.3g/㎝3The bending strength is 250 MPa-480 MPa, and the resistivity is 10 mu omega-300 mu omega-m.
By adopting the technical scheme, the invention better realizes the aim of the invention, the ceramic powder and the lubricant comprising graphite powder or graphene are introduced into the carbon fiber preform in a physical mode at room temperature, and the carbon-ceramic composite material heater is prepared after vapor deposition, and the carbon-ceramic composite material heater has the characteristics of simple process, short production period, low preparation cost, good conductivity and the like; the added lubricant reduces the abrasion of the ceramic powder to the needle and the abrasion to the fiber during the needling, simultaneously, in the needling process, the ceramic slurry is injected at intervals, so that the damage of the silicon carbide powder to the fiber is greatly reduced, the excessive abrasion to the needle is not generated, and the fiber content of the carbon/carbon blank body is not influenced because the needle is firstly needled to a certain thickness and then injected; the prepared carbon-ceramic composite material heater has the open porosity of 1-9% and the density of 1.5g/cm3～2.3g/㎝3The bending strength is 250MPa to 480MPa, and the resistivity is 10 mu omega to 300 mu omega; the carbon-ceramic composite material has a thermal expansion coefficient closer to that of silicon carbide and good thermal shock resistance, the resistivity of the carbon-ceramic composite material can be well controlled by adjusting the ceramic content in the carbon-ceramic composite material, and meanwhile, the carbon-ceramic composite material heater with required resistance can be obtained by changing the structure of the carbon-ceramic composite material heater, and the service life of the heater in a single crystal thermal field is also greatly prolonged.
Drawings
FIG. 1 is a schematic structural view of the lancing mechanism of the present invention;
FIG. 2 is a cross-sectional view A-A of FIG. 1;
FIG. 3 is a schematic structural view of examples 1 and 4 of the present invention;
FIG. 4 is a 2000 times magnified electron micrograph of 5 μm silicon carbide powder used in example 1 of the present invention;
FIG. 5 is a 50 times magnified electron microscope image of the cross section of the carbon ceramic composite heater according to example 1 of the present invention;
FIG. 6 is a schematic structural view of embodiment 2 of the present invention;
FIG. 7 is a schematic structural view of embodiment 3 of the present invention;
fig. 8 is a schematic structural view of embodiments 5 and 6 of the present invention.
Detailed Description
The invention is further explained below with reference to the drawings and examples.
Example 1:
a preparation method of a carbon-ceramic composite material heater comprises the following steps:
⑴, preparing ceramic slurry, namely, mixing ceramic powder, a dispersant and a solvent uniformly by stirring and ball milling, adjusting the pH value of the solution, and preparing suspended ceramic slurry, wherein the ceramic slurry also comprises a lubricant, the lubricant is one of graphite powder or graphene, and the mass ratio of the ceramic powder to the lubricant is 1: 0.1-0.3, the pH value of the prepared ceramic slurry is 11.8-12.0, the solid content of the ceramic powder is 10-30%, and the viscosity is 50-200 mPa.S;
in step ⑴, the ceramic powder is one or more of silicon carbide, silicon nitride or boron carbide, the particle size of the ceramic powder is 0.1-10 μm, the purity is 99.0%, the dispersant is one of polyvinyl alcohol, polyethylene glycol, epoxy resin or phenolic resin, the solvent is distilled water, and the mass ratio of the ceramic powder to the dispersant to the solvent is 1: 0.05-0.1: 2.23-8.95.
In step ⑴, the particle size of the graphite powder is 1-10 μm, the purity of the graphite powder is 99%, the particle size of the graphene is 35-50 μm, and the purity of the graphene is 95%.
In step ⑴, the pH value is adjusted by using 30% hydrochloric acid and acrylamide or liquid ammonia as an alkali.
⑵ preparing a wet blank of the carbon ceramic composite heater, namely alternately laminating and needling a carbon fiber mesh tire and carbon fiber cloth into a carbon/carbon preform according to a drawing, needling the carbon/carbon preform by a needling mechanism, wherein the needling mechanism comprises a needle seat, and an injection needle and a needling needle are arranged on the needle seat;
in step ⑵, the carbon fiber cloth is a unidirectional cloth or a mixed cloth with an area density of 500g/m2～1400g/m2(ii) a The areal density of the net tyre is 30g/m2～130g/m2(ii) a The needling depth is 6-25 mm, and the needling density is 4 times/cm28 times/cm2Injection density of 1 times/cm 22 times/cm2(ii) a The number ratio of the injection needles to the acupuncture needles is 1: 4-6, wherein the length of the injection needle is longer than that of the acupuncture needle by 2 +/-0.1 mm.
In step ⑵, the pressure during injection is 0.25MPa to 0.45MPa, and the injection amount of the ceramic slurry is 2.0 g/cm3～4.67g/㎝3The introduction amount of the ceramic powder in the carbon-ceramic composite material heater wet blank is 0.2 g/cm3～1.4g/㎝3。
⑶, preparing a dry blank of the carbon-ceramic composite material heater, namely, putting the wet blank of the carbon-ceramic composite material heater prepared in the step ⑵ into an environment with the temperature of 100-200 ℃ for processing for 6-24 h to prepare the dry blank of the carbon-ceramic composite material heater, wherein the density of the dry blank of the carbon-ceramic composite material heater is 0.6 g/cm3～2.0g/㎝3；
⑷, rough machining, namely rough machining is carried out on the carbon-ceramic composite material heater dry blank according to a drawing, and allowance required by subsequent machining is reserved;
⑸ vapor deposition, namely putting the carbon-ceramic composite material heater dry blank prepared in the step ⑷ into a vapor deposition furnace for vapor deposition;
in step ⑸, during vapor deposition, natural gas or methane or propane is used as a raw material, the deposition pressure is 1 kPa-3 kPa, and the deposition temperature is 950 ℃ -1200 ℃;
⑹ finish machining, repeating the steps ⑷ and ⑸ until the deposition density is set, and finish machining according to the drawingPreparing a carbon-ceramic composite material heater; the open porosity of the carbon-ceramic composite material heater is 1-9%, and the density is 1.5g/cm3～2.3g/㎝3The bending strength is 250 MPa-480 MPa, and the resistivity is 10 mu omega-300 mu omega-m.
In order to prevent corrosion and prolong the service life, after the step ⑹, the method carries out a step ⑺, and the carbon-ceramic composite material heater is put into a silicon carbide CVD deposition furnace for carrying out surface deposition of a SiC coating, wherein the thickness of the coating is 5-2000 mu m.
In step ⑺, during vapor deposition, trichloromethylsilane is used as the raw material, hydrogen is used as the carrier gas, argon is used as the diluent gas, the deposition pressure is 1 kPa-3 kPa, and the deposition temperature is 900 ℃ -1250 ℃.
The carbon-ceramic composite material heater prepared by the method is characterized in that the open porosity of the heater is 1-9%, and the density is 1.5g/cm3～2.3g/㎝3The bending strength is 250 MPa-480 MPa, and the resistivity is 10 mu omega-300 mu omega-m.
As shown in fig. 1 and 2, the acupuncture mechanism of the invention comprises a needle seat 1, wherein an injection needle 3 and an acupuncture needle 2 are arranged on the needle seat 1; when the carbon/carbon preform is needled, fibers in the Z-axis direction are formed by the needling needles 2, and at the same time, the ceramic slurry is injected into the carbon/carbon preform by the injection needles 3.
The number ratio of the injection needle 3 to the acupuncture needle 2 is 1: 4-6, the length of the injection needle 3 is longer than that of the acupuncture needle 2 by 2 +/-0.1 mm.
The carbon-ceramic composite material heater comprises at least 2 heating rings 7, at least 2 supporting legs 5 and a connecting bolt 4 for connecting the two; the heating ring 7 is a cylinder, and a heating ring connecting plane and a connecting screw hole are processed at the assembly part of the heating ring 7 and the supporting leg 5; the supporting leg 5 comprises a heating ring connecting end and an electrode connecting end, is integrally L-shaped, a supporting leg connecting plane for assembling the heating ring 7 is processed on the heating ring connecting end, a connecting through hole for allowing the connecting bolt 4 to penetrate through is formed in the supporting leg connecting plane, a boss 8 for supporting the heating ring 7 is arranged below the supporting leg connecting plane, and the heating ring 7 is installed on the heating ring connecting end through the connecting bolt 4; the electrode connecting end is provided with a through hole 6 for installing an electrode; the distribution gradient of the axial temperature of the heater is adjusted by changing the number and the height of the heating rings 7 and the distance between the adjacent heating rings 7.
In this example, silicon carbide with a particle size of 5 μm, polyvinyl alcohol, and distilled water were mixed in a mass ratio of 1: 0.1: 3.9, adding graphite powder with the particle size of 1 mu m, and mixing the materials in percentage by mass: and (3) adding acrylamide to adjust the pH value to 12 after the graphite powder is 1:0.2, and then carrying out ball milling for 2 hours at the rotating speed of 120r/min to prepare suspended ceramic slurry, wherein the solid content of silicon carbide in the ceramic slurry is 20% and the viscosity is 100 mPa.S.
Alternately stacking carbon fiber cloth and net blank on the foam tool in sequence and needling, wherein the carbon fiber cloth is interwoven fabric with the surface density of 1000g/m2The surface density of the net tire is 130g/m2The number ratio of the injection needle 3 to the acupuncture needle 2 is 1: 4, the length of the injection needle 3 is longer than that of the needle 2 by 2 +/-0.1 mm, the needle depth is 6 mm, and the needle density is 8 times/cm2Injection density of 2 times/cm2When stacking, the included angle of the carbon fibers of the two adjacent layers of carbon fiber cloth is 45 degrees, when the thickness of the blank body reaches 2 mm, starting to perform needling and injecting, forming fibers in the Z-axis direction by a needling needle 2, injecting the ceramic slurry prepared in the step ⑴ into the carbon/carbon prefabricated body by an injection needle 3, wherein the pressure during injection is 0.3MPa, and the injection amount is 4.0 g/cm3The introduction amount of the silicon carbide in the wet preform is 0.8 g/cm3. The above operations are repeated to reach the designed thickness, and finally a cylinder-type carbon-ceramic composite wet blank with the thickness of 30 mm, a square frame-type carbon-ceramic composite wet blank with the thickness of 60 mm and a plate-type carbon-ceramic composite wet blank with the thickness of 45 mm are prepared (in the embodiment, the processes of the three are the same). The wet carbon-ceramic composite material blank is put into an oven to be baked for 12 hours at the temperature of 200 ℃ to prepare a dry carbon-ceramic composite material blank, and the density of the dry carbon-ceramic composite material blank is 1.38 g/cm3。
Roughly processing the carbon-ceramic composite material dry blank according to a drawing, and reserving allowance required by subsequent processing;
and (3) putting the rough-processed carbon-ceramic composite material dry blank into a CVI furnace for vapor deposition, wherein the specific process comprises the following steps: heating the CVI furnace to 1100 DEG CThe temperature is kept for 1h at 300 ℃ and 600 ℃ respectively, the whole heating rate is 5 ℃/min, the deposition time is 160h at 1100 ℃, the raw material for deposition is natural gas, and the deposition pressure is 1500 Pa. After twice deposition, the required density is reached to 1.9g/cm3。
As shown in fig. 3, the cylindrical carbon ceramic composite material is processed into the heating ring 7 with the required height, mirror-symmetrical connection planes are milled, and connection screw holes are drilled. The square frame type carbon ceramic composite material is processed into two identical supporting legs 5, and a connecting through hole for passing through a connecting bolt 4, a boss 8 for supporting a heating ring 7 and a through hole 6 for assembling an electrode are milled at a required position. The plate-type carbon ceramic composite material is processed into 12 connecting bolts 4.
In the embodiment, 3 heating coils 7 are combined, and the heating coils 7 are respectively fastened and connected with the supporting legs 5 through 2 connecting bolts 4. When viewed from the near to the far from the electrode connecting end, the heights of the heating rings 7 are sequentially 30 mm, 30 mm and 50 mm, and the gap heights between the adjacent heating rings 7 are sequentially 130 mm and 90 mm.
The density of the carbon-ceramic composite material heater prepared by the embodiment is 1.9g/cm34.8% of open porosity, 320MPa of bending strength, 120 [ mu ] omega.m of resistivity and 2.6 x 10 of coefficient of thermal expansion-6/℃。
In order to prevent corrosion and prolong the service life, the prepared carbon-ceramic composite material heater is put into a silicon carbide CVD furnace, the temperature is 1200 ℃, the pressure is 1000Pa, and the SiC coating with the thickness of 100 mu m is obtained after deposition for 15 h.
The heater structure is changed in the embodiment, the heater structure is combined and formed, and the distribution gradient of the axial temperature of the heater is adjusted by changing the number and the height of the heating rings 7 and the distance between the adjacent heating rings 7.
As can be seen from FIG. 4, the silicon carbide powder has uniform particle size but is not spherical, and the edges and corners can be removed by ball milling at the later stage, so that the injection by a syringe needle is facilitated.
As can be seen from fig. 5, the dark areas are carbon fibers and deposited carbon, and the light areas are silicon carbide; the silicon carbide is uniformly distributed in the carbon-ceramic composite material, is microcosmically compact, has low porosity, excellent mechanical property, wear resistance, oxidation resistance and corrosion resistance, and greatly prolongs the service life of the material in a thermal field. The service life of the heater prepared from the carbon-carbon composite material in the single crystal furnace is 1-2 months. The service life of the carbon-ceramic composite material heater prepared by the invention in a single crystal furnace is 5-6 months.
According to the invention, ceramic powder and a lubricant comprising graphite powder or graphene are introduced into the carbon fiber preform at room temperature in a physical manner, and the carbon-ceramic composite material heater is prepared after vapor deposition, and has the characteristics of simple process, short production period, low preparation cost, good conductivity and the like; the added lubricant reduces the abrasion of the ceramic powder to the needle and the abrasion to the fiber during needling, fills the pores among the carbon fibers, further reduces the open porosity of the carbon-ceramic composite material heater, and also improves the bending strength of the carbon-ceramic composite material heater; meanwhile, in the needling process, the damage of silicon carbide powder to fibers is greatly reduced by injecting ceramic slurry at intervals, excessive abrasion to needling needles is avoided, and the fiber content of the carbon/carbon blank body is not influenced because the silicon carbide powder is needled to a certain thickness and then injected; the prepared carbon-ceramic composite material heater has the open porosity of 1-9% and the density of 1.5g/cm3～2.3g/㎝3The bending strength is 250MPa to 480MPa, and the resistivity is 10 mu omega to 300 mu omega; the carbon-ceramic composite material disclosed by the invention has a thermal expansion coefficient closer to that of silicon carbide and good thermal shock resistance, and the resistivity of the carbon-ceramic composite material can be well controlled by adjusting the ceramic content in the carbon-ceramic composite material.
Example 2:
in this example, silicon carbide with a particle size of 5 μm, polyvinyl alcohol, and distilled water were mixed in a mass ratio of 1: 0.05: 8.95, adding graphite powder with the particle size of 1 mu m, and mixing the materials in percentage by mass: and (3) adding acrylamide to adjust the pH value to 12 after the graphite powder is 1:0.2, and then carrying out ball milling for 2 hours at the rotating speed of 120r/min to prepare suspended ceramic slurry, wherein the solid content of silicon carbide in the ceramic slurry is 10% and the viscosity is 50 mPa.S.
Alternately stacking carbon fiber cloth and net blank on porous metal net and needling to obtain carbon fiber clothThe fiber cloth is interwoven fabric with surface density of 1000g/m2The surface density of the net tire is 100g/m2The number ratio of the injection needle 3 to the acupuncture needle 2 is 1: 4, the length of the injection needle 3 is longer than that of the needle 2 by 2 +/-0.1 mm, the needle depth is 6 mm, and the needle density is 8 times/cm2Injection density of 2 times/cm2When stacking, the included angle of the carbon fibers of the two adjacent layers of carbon fiber cloth is 45 degrees, when the thickness of the blank body reaches 2 mm, starting to perform needling and injecting, forming fibers in the Z-axis direction by a needling needle 2, injecting the ceramic slurry prepared in the step ⑴ into the carbon/carbon prefabricated body by an injection needle 3, wherein the pressure during injection is 0.25MPa, and the injection amount is 2.0 g/cm3The introduction amount of the silicon carbide in the wet preform is 0.2 g/cm3. And repeating the operation, and finally preparing the wet blank of the cylindrical carbon-ceramic composite material heater with the step, wherein the cylinder thickness is 30 mm, and the step thickness is 60 mm. Putting the wet blank of the carbon-ceramic composite material heater into an oven to be baked for 12h at 200 ℃ to prepare a dry blank of the carbon-ceramic composite material heater, wherein the density of the dry blank of the carbon-ceramic composite material heater is 0.7 g/cm3。
Roughly processing a dry blank of the carbon-ceramic composite material heater according to a drawing, and reserving allowance required by subsequent processing;
putting the rough processed dry blank of the carbon-ceramic composite material heater into a CVI furnace for vapor deposition, wherein the specific process comprises the following steps: heating a CVI furnace to 1100 ℃, keeping the temperature for 1h at the temperature of 300 ℃ and 600 ℃, wherein the whole heating rate is 5 ℃/min, the deposition time at 1100 ℃ is 100h, the raw material for deposition is natural gas, and the deposition pressure is 1500 Pa. After one deposition, the required density is 1.5g/cm3。
As shown in fig. 6, the step position is machined in the shape of a mirror-symmetrical electrode connection end, and a through hole 6 for fitting the electrode is milled. And milling axial grooves which are distributed in sequence and only penetrate through the upper end surface or the lower end surface of the cylinder body according to a required position.
The heating area of the heater in this embodiment has 16 grooves and 4 electrode connecting ends.
The density of the carbon-ceramic composite material heater prepared by the embodiment is 1.5g/cm3The open porosity is 9%, the bending strength is 250MPa, the resistivity is 60 mu omega, m, and the thermal expansion is realizedCoefficient of expansion of 1.5X 10-6/℃。
In order to prevent corrosion and prolong the service life, the prepared carbon-ceramic composite material heater is put into a silicon carbide CVD furnace, the temperature is 1100 ℃, the pressure is 1000Pa, and the SiC coating with the thickness of 30 mu m is obtained after deposition for 5 h.
The heater structure of this embodiment is traditional structure, and the integrated into one piece.
The same as in example 1.
Example 3:
the carbon-ceramic composite material heater is a cylinder with a connecting part, at least 2 heating rings 7 are arranged on the cylinder in parallel along the axis, adjacent heating rings 7 are connected through a connecting block 9, the connecting block 9 is L-shaped, a through hole 6 for installing a power electrode is processed at one end of the connecting block 9, namely the connecting part, and the connecting block 9 and the heating rings 7 are integrally formed; the distribution gradient of the axial temperature of the heater is adjusted by changing the number and the height of the heating rings 7 and the distance between the adjacent heating rings 7.
In this example, silicon carbide with a particle size of 5 μm, polyvinyl alcohol, and distilled water were mixed in a mass ratio of 1: 0.1: 2.23, adding graphite powder with the particle size of 1 mu m, and mixing the materials in percentage by mass: and (3) adding acrylamide to adjust the pH value to 12 after the graphite powder is 1:0.2, and then carrying out ball milling for 2 hours at the rotating speed of 120r/min to prepare suspended ceramic slurry, wherein the solid content of silicon carbide in the ceramic slurry is 30% and the viscosity is 200 mPa.S.
Alternately stacking carbon fiber cloth and net blank on porous metal net in turn and needling, wherein the carbon fiber cloth is interwoven fabric with surface density of 1400g/m2The surface density of the net tire is 130g/m2The number ratio of the injection needle 3 to the acupuncture needle 2 is 1: 4, the length of the injection needle 3 is longer than that of the needle 2 by 2 +/-0.1 mm, the needle depth is 6 mm, and the needle density is 8 times/cm2Injection density of 2 times/cm2When stacking, the included angle of the carbon fibers of the two adjacent layers of carbon fiber cloth is 45 degrees, during needling, when the thickness of the blank body reaches 2 mm, needling is started and injection is carried out, fibers in the Z-axis direction are formed by a needling needle 2, the ceramic slurry prepared in the step ⑴ is injected into the carbon/carbon prefabricated body by an injection needle 3, the pressure during injection is 0.45MPa, and the injection amount isIs 4.67 g/cm3The introduction amount of the silicon carbide in the wet preform is 1.4 g/cm3. And repeating the operations to finally obtain the wet blank of the cylindrical carbon-ceramic composite material heater with the step (namely the connecting part), wherein the cylinder thickness is 30 mm, and the step thickness is 60 mm. Putting the wet blank of the carbon-ceramic composite material heater into an oven to be baked for 12h at 200 ℃ to prepare a dry blank of the carbon-ceramic composite material heater, wherein the density of the dry blank of the carbon-ceramic composite material heater is 1.98 g/cm3。
Roughly processing the dry blank of the carbon-ceramic composite material heater according to a drawing, and reserving allowance required by subsequent processing;
putting the rough processed dry blank of the carbon-ceramic composite material heater into a CVI furnace for vapor deposition, wherein the specific process comprises the following steps: heating a CVI furnace to 1100 ℃, keeping the temperature for 1h at the temperature of 300 ℃ and 600 ℃, wherein the whole heating rate is 5 ℃/min, the deposition time at 1100 ℃ is 130h, the raw material for deposition is natural gas, and the deposition pressure is 1500 Pa. After twice deposition, the required density is reached to 2.3g/cm3。
As shown in fig. 7, the step (i.e., the connecting portion) is machined in the shape of the electrode connecting end in mirror symmetry, and a through hole 6 for fitting the electrode is milled. The cylinder body close to the electrode connecting end is processed into a supporting leg which has the same width as the electrode connecting end and is connected with the electrode connecting end and is used for supporting and connecting the heating coil 7, and the shape of the supporting leg extends to the non-step end face of the cylinder to form a connecting block 9. The remaining barrel section is shaped in the desired position as a hot ring 7. The end face of the heating coil farthest from the electrode connecting end is also the end face of the cylinder body of the whole heater.
In this embodiment, there are 4 heating coils 7 in total. Viewed from near to far from the electrode connecting end, the heights of the heating rings 7 are sequentially 30 mm, 37.5 mm and 60 mm, and the gap heights between the adjacent heating rings 7 are sequentially 112.5 mm, 45 mm and 45 mm.
The density of the carbon-ceramic composite material heater prepared by the embodiment is 2.3g/cm 31% open porosity, bending strength of 450MPa, resistivity of 300 [ mu ] omega, and thermal expansion coefficient of 3.6 × 10-6/℃。
In order to prevent corrosion and prolong the service life, the prepared carbon-ceramic composite material heater is put into a silicon carbide CVD furnace, the temperature is 1250 ℃, the pressure is 3000Pa, and the SiC coating with the thickness of 1500 mu m is obtained after deposition for 100 h.
The structure of the heater is changed and the heater is integrally formed, and the distribution gradient of the axial temperature of the heater is adjusted by changing the number and the height of the heating rings 7 and the distance between the adjacent heating rings 7.
The same as in example 1.
Example 4:
in this example, silicon carbide with a particle size of 5 μm, polyvinyl alcohol, and distilled water were mixed in a mass ratio of 1: 0.1: 3.9, adding graphite powder with the particle size of 1 mu m, and mixing the materials in percentage by mass: and (3) adding acrylamide to adjust the pH value to 12 after the graphite powder is 1:0.1, and then carrying out ball milling for 2 hours at the rotating speed of 120r/min to prepare suspended ceramic slurry, wherein the solid content of silicon carbide in the ceramic slurry is 20% and the viscosity is 95 mPa.S.
Alternately stacking carbon fiber cloth and net blank on the foam tool in sequence and needling, wherein the carbon fiber cloth is interwoven fabric with the surface density of 1000g/m2The surface density of the net tire is 130g/m2The number ratio of the injection needle 3 to the acupuncture needle 2 is 1: 4, the length of the injection needle 3 is longer than that of the needle 2 by 2 +/-0.1 mm, the needle depth is 6 mm, and the needle density is 8 times/cm2Injection density of 2 times/cm2When stacking, the included angle of the carbon fibers of the two adjacent layers of carbon fiber cloth is 45 degrees, when the thickness of the blank body reaches 2 mm, starting to perform needling and injecting, forming fibers in the Z-axis direction by a needling needle 2, injecting the ceramic slurry prepared in the step ⑴ into the carbon/carbon prefabricated body by an injection needle 3, wherein the pressure during injection is 0.3MPa, and the injection amount is 4.0 g/cm3The introduction amount of the silicon carbide in the wet preform is 0.8 g/cm3. The above operations are repeated to reach the designed thickness, and finally, a cylindrical carbon-ceramic composite wet blank with the thickness of 30 mm, a square frame carbon-ceramic composite wet blank with the thickness of 60 mm and a plate carbon-ceramic composite wet blank with the thickness of 45 mm are prepared (in the embodiment, the processes of the three are the same). The wet carbon-ceramic composite material blank is put into an oven to be baked for 12 hours at the temperature of 200 ℃ to prepare a dry carbon-ceramic composite material blank, and the density of the dry carbon-ceramic composite material blank is 1.35 g/cm3。
Roughly processing the carbon-ceramic composite material dry blank according to a drawing, and reserving a processing allowance;
and (3) putting the rough-processed carbon-ceramic composite material dry blank into a CVI furnace for vapor deposition, wherein the specific process comprises the following steps: heating a CVI furnace to 1100 ℃, keeping the temperature for 1h at the temperature of 300 ℃ and 600 ℃, wherein the whole heating rate is 5 ℃/min, the deposition time at 1100 ℃ is 100h, the raw material for deposition is natural gas, and the deposition pressure is 1500 Pa. After one deposition, the required density is 1.86g/cm3。
As shown in fig. 3, the cylindrical carbon ceramic composite material is processed into the heating ring 7 with the required height, mirror-symmetrical connection planes are milled, and connection screw holes are drilled. The square frame type carbon ceramic composite material is processed into two identical supporting legs 5, and a connecting through hole for passing through a connecting bolt 4, a boss 8 for supporting a heating ring 7 and a through hole 6 for assembling an electrode are milled at a required position. The plate material is machined into 12 attachment bolts 4.
In the embodiment, 3 heating rings 7 are combined together, and each heating ring 7 is fixedly connected with the supporting foot 5 through 2 connecting bolts 4. When viewed from the near to the far from the electrode connecting end, the heights of the heating rings 7 are sequentially 30 mm, 30 mm and 55 mm, and the gap heights between the adjacent heating rings 7 are sequentially 130 mm and 90 mm.
The density of the carbon-ceramic composite material heater prepared by the embodiment is 1.86g/cm34.9% of open porosity, 320MPa of bending strength, 174 mu omega m of resistivity and 2.58 multiplied by 10 of coefficient of thermal expansion-6/℃。
In order to prevent corrosion and prolong the service life, the prepared carbon-ceramic composite material heater is put into a silicon carbide CVD furnace, the temperature is 1200 ℃, the pressure is 1000Pa, and the SiC coating with the thickness of 100 mu m is obtained after deposition for 15 h.
The heater structure is changed in the embodiment, the heater structure is combined and formed, and the distribution gradient of the axial temperature of the heater is adjusted by changing the number and the height of the heating rings 7 and the distance between the adjacent heating rings 7.
The same as in example 1.
Example 5:
in this example, silicon carbide with a particle size of 5 μm, polyvinyl alcohol, and distilled water were mixed in a mass ratio of 1: 0.1: 3.9, adding graphite powder with the particle size of 1 mu m, and mixing the materials in percentage by mass: and (3) adding acrylamide to adjust the pH value to 12, and then carrying out ball milling for 2 hours at the rotating speed of 120r/min to prepare suspended ceramic slurry, wherein the solid content of silicon carbide in the ceramic slurry is 20% and the viscosity is 120 mPa.S.
Alternately stacking carbon fiber cloth and net blank on the foam tool in sequence and needling, wherein the carbon fiber cloth is interwoven fabric with the surface density of 1000g/m2The surface density of the net tire is 130g/m2The number ratio of the injection needle 3 to the acupuncture needle 2 is 1: 4, the length of the injection needle 3 is longer than that of the needle 2 by 2 +/-0.1 mm, the needle depth is 6 mm, and the needle density is 8 times/cm2Injection density of 2 times/cm2When stacking, the included angle of the carbon fibers of the two adjacent layers of carbon fiber cloth is 45 degrees, when the thickness of the blank body reaches 2 mm, starting to perform needling and injecting, forming fibers in the Z-axis direction by a needling needle 2, injecting the ceramic slurry prepared in the step ⑴ into the carbon/carbon prefabricated body by an injection needle 3, wherein the pressure during injection is 0.3MPa, and the injection amount is 4.0 g/cm3The introduction amount of the silicon carbide in the wet preform is 0.8 g/cm3. The above operations are repeated to reach the designed thickness, and finally, a cylinder-type carbon-ceramic composite wet blank with the thickness of 30 mm, a frame-type carbon-ceramic composite wet blank with the thickness of 60 mm and a plate-type carbon-ceramic composite wet blank with the thickness of 45 mm are prepared (in the embodiment, the processes of the three are the same). The wet carbon-ceramic composite material blank is put into an oven to be baked for 12 hours at the temperature of 200 ℃ to prepare a dry carbon-ceramic composite material blank, and the density of the dry carbon-ceramic composite material blank is 1.40 g/cm3。
Roughly processing the carbon-ceramic composite material dry blank according to a drawing, and reserving a processing allowance;
and (3) putting the rough-processed carbon-ceramic composite material dry blank into a CVI furnace for vapor deposition, wherein the specific process comprises the following steps: heating a CVI furnace to 1100 ℃, keeping the temperature for 1h at the temperature of 300 ℃ and 600 ℃, wherein the whole heating rate is 5 ℃/min, the deposition time at 1100 ℃ is 200h, the raw material for deposition is natural gas, and the deposition pressure is 1500 Pa. Depositing twiceThen the required density of 1.93g/cm is achieved3。
As shown in fig. 8, axial grooves which penetrate only the upper end surface or the lower end surface and are distributed in sequence are milled on the cylindrical carbon-ceramic composite material according to a required position, a connecting plane is milled by taking an extension line of a certain groove as a center, and a connecting screw hole is drilled. The same connecting plane and connecting screw holes are processed at other three points which are uniformly distributed in the circumferential direction. The square frame type carbon ceramic composite material is processed into four same supporting legs 5, and connecting through holes for passing through connecting bolts 4 and through holes 6 for assembling electrodes are milled at required positions. The plate-type carbon ceramic composite material is processed into 16 connecting bolts 4.
The heating area of the heater in the embodiment has 16 grooves in total, 4 supporting legs 5 are combined, and each supporting leg 5 is fastened and connected with the heating area through 4 connecting bolts 4.
The density of the carbon-ceramic composite material heater prepared by the embodiment is 1.93g/cm34.5% of open porosity, 328MPa of bending strength, 81 mu omega of resistivity and 3.0 multiplied by 10 of coefficient of thermal expansion-6/℃。
In order to prevent corrosion and prolong the service life, the prepared carbon-ceramic composite material heater is put into a silicon carbide CVD furnace, the temperature is 1200 ℃, the pressure is 1000Pa, and the SiC coating with the thickness of 100 mu m is obtained after deposition for 15 h.
The heater structure of the embodiment is a traditional structure and is formed by combination.
The same as in example 1.
Example 6:
in this example, silicon carbide with a particle size of 5 μm, polyvinyl alcohol, and distilled water were mixed in a mass ratio of 1: 0.1: 3.9, adding graphene with the particle size of 35 μm, wherein the mass ratio of silicon carbide: and (3) adding acrylamide to adjust the pH value to 12 when the ratio of graphene is 1:0.1, then carrying out ball milling for 2 hours at a rotation speed of 120r/min, and preparing suspended ceramic slurry, wherein the solid content of silicon carbide in the ceramic slurry is 20% and the viscosity is 110 mPa.S.
Alternately stacking carbon fiber cloth and net blank on the foam tool in sequence and needling, wherein the carbon fiber cloth is interwoven fabric with the surface density of 1000g/m2The surface density of the net tire is 130g/m2The number ratio of the injection needle 3 to the acupuncture needle 2 is 1: 4, the length of the injection needle 3 is longer than that of the needle 2 by 2 +/-0.1 mm, the needle depth is 6 mm, and the needle density is 8 times/cm2Injection density of 2 times/cm2When stacking, the included angle of the carbon fibers of the two adjacent layers of carbon fiber cloth is 45 degrees, when the thickness of the blank body reaches 2 mm, starting to perform needling and injecting, forming fibers in the Z-axis direction by a needling needle 2, injecting the ceramic slurry prepared in the step ⑴ into the carbon/carbon prefabricated body by an injection needle 3, wherein the pressure during injection is 0.3MPa, and the injection amount is 4.0 g/cm3The introduction amount of the silicon carbide in the wet preform is 0.8 g/cm3. The above operations are repeated to reach the designed thickness, and finally, a cylindrical carbon-ceramic composite wet blank with the thickness of 30 mm, a square frame carbon-ceramic composite wet blank with the thickness of 60 mm and a plate carbon-ceramic composite wet blank with the thickness of 45 mm are prepared (in the embodiment, the processes of the three are the same). The wet carbon-ceramic composite material blank is put into an oven to be baked for 12 hours at the temperature of 200 ℃ to prepare a dry carbon-ceramic composite material blank, and the density of the dry carbon-ceramic composite material blank is 1.38 g/cm3。
Roughly processing the carbon-ceramic composite material dry blank according to a drawing, and reserving a processing allowance;
and (3) putting the rough-processed carbon-ceramic composite material dry blank into a CVI furnace for vapor deposition, wherein the specific process comprises the following steps: heating a CVI furnace to 1100 ℃, keeping the temperature for 1h at the temperature of 300 ℃ and 600 ℃, wherein the whole heating rate is 5 ℃/min, the deposition time at 1100 ℃ is 160h, the raw material for deposition is natural gas, and the deposition pressure is 1500 Pa. After twice deposition, the required density is reached to be 1.85g/cm3。
As shown in fig. 8, axial grooves which penetrate only the upper end surface or the lower end surface and are distributed in sequence are milled on the cylindrical carbon-ceramic composite material according to a required position, a connecting plane is milled by taking an extension line of a certain groove as a center, and a connecting screw hole is drilled. The same connecting plane and connecting screw holes are processed at other three points which are uniformly distributed in the circumferential direction. The square frame type carbon ceramic composite material is processed into four same supporting legs 5, and connecting through holes for passing through connecting bolts 4 and through holes 6 for assembling electrodes are milled at required positions. The plate-type carbon ceramic composite material is processed into 16 connecting bolts 4.
The heating area of the heater in the embodiment has 16 grooves in total, 4 supporting legs 5 are combined, and each supporting leg 5 is fastened and connected with the heating area through 4 connecting bolts 4.
The density of the carbon-ceramic composite material heater prepared by the embodiment is 1.95g/cm34.7% of open porosity, 380MPa of bending strength, 25 mu omega of resistivity and 2.0 multiplied by 10 of coefficient of thermal expansion-6/℃。
In order to prevent corrosion and prolong the service life, the prepared carbon-ceramic composite material heater is put into a silicon carbide CVD furnace, the temperature is 1200 ℃, the pressure is 1000Pa, and the SiC coating with the thickness of 100 mu m is obtained after deposition for 15 h.
The heater structure of the embodiment is a traditional structure and is formed by combination.
The same as in example 1.
As is clear from examples 1, 2 and 3, the resistivity increased and the thermal expansion coefficient increased as the silicon carbide content increased. As is clear from examples 1, 4 and 5, the resistivity decreased and the thermal expansion coefficient increased as the content of graphite powder increased. As is clear from examples 1 and 6, the incorporation of graphene further improves the flexural strength of the material and reduces the specific resistance of the material, compared to graphite powder.

Claims (10)

1. A preparation method of a carbon-ceramic composite material heater is characterized by comprising the following steps:
⑴, preparing ceramic slurry, namely, mixing ceramic powder, a dispersant and a solvent uniformly by stirring and ball milling, adjusting the pH value of the solution, and preparing suspended ceramic slurry, wherein the ceramic slurry also comprises a lubricant, the lubricant is one of graphite powder or graphene, and the mass ratio of the ceramic powder to the lubricant is 1: 0.1-0.3, the pH value of the prepared ceramic slurry is 11.8-12.0, the solid content of the ceramic powder is 10-30%, and the viscosity is 50-200 mPa.S;
⑵ preparing a wet blank of the carbon ceramic composite heater, namely alternately laminating and needling a carbon fiber mesh tire and carbon fiber cloth into a carbon/carbon preform according to a drawing, needling the carbon/carbon preform by a needling mechanism, wherein the needling mechanism comprises a needle seat, and an injection needle and a needling needle are arranged on the needle seat;
⑶, preparing a dry blank of the carbon-ceramic composite material heater, namely, putting the wet blank of the carbon-ceramic composite material heater prepared in the step ⑵ into an environment with the temperature of 100-200 ℃ for processing for 6-24 h to prepare the dry blank of the carbon-ceramic composite material heater, wherein the density of the dry blank of the carbon-ceramic composite material heater is 0.6 g/cm3～2.0g/㎝3；
⑷, rough machining, namely rough machining is carried out on the carbon-ceramic composite material heater dry blank according to a drawing, and allowance required by subsequent machining is reserved;
⑸ vapor deposition, namely putting the carbon-ceramic composite material heater dry blank prepared in the step ⑷ into a vapor deposition furnace for vapor deposition;
⑹, repeating the steps ⑷ and ⑸ to the set deposition density, and carrying out finish machining according to a drawing to manufacture the carbon-ceramic composite material heater, wherein the open porosity of the carbon-ceramic composite material heater is 1-9%, and the density is 1.5g/cm3～2.3g/㎝3The bending strength is 250 MPa-480 MPa, and the resistivity is 10 mu omega-300 mu omega-m.
2. The preparation method of the carbon-ceramic composite material heater as claimed in claim 1, wherein after the step ⑹, the step ⑺ of corrosion prevention treatment is carried out, and the carbon-ceramic composite material heater is placed in a silicon carbide CVD furnace to carry out surface deposition of a SiC coating, wherein the thickness of the coating is 5 μm to 2000 μm.
3. The method as claimed in claim 2, wherein in the step ⑺, the carbon-ceramic composite material heater is prepared by vapor deposition using trichloromethylsilane as raw material, hydrogen as carrier gas, argon as diluent gas, deposition pressure is 1 kPa-3 kPa, and deposition temperature is 900 ℃ -1250 ℃.
4. The preparation method of the carbon-ceramic composite material heater according to claim 1, wherein in step ⑴, the ceramic powder is one or more of silicon carbide, silicon nitride and boron carbide, the ceramic powder has a particle size of 0.1-10 μm and a purity of 99.0%, the dispersing agent is one of polyvinyl alcohol, polyethylene glycol, epoxy resin and phenolic resin, the solvent is distilled water, and the mass ratio of the ceramic powder to the dispersing agent to the solvent is 1: 0.05-0.1: 2.23-8.95.
5. The preparation method of the carbon-ceramic composite material heater as claimed in claim 1, wherein in the step ⑴, the particle size of the graphite powder is 1-10 μm, the purity of the graphite powder is 99%, the particle size of the graphene is 35-50 μm, and the purity of the graphene is 95%.
6. The method of claim 1, wherein in step ⑴, the pH is adjusted by using 30% hydrochloric acid and the alkali is acrylamide or liquid ammonia.
7. The method as claimed in claim 1, wherein in step ⑵, the carbon fiber cloth is a unidirectional cloth or a mixed cloth with an area density of 500g/m2～ 1400g/m2(ii) a The areal density of the net tyre is 30g/m2～130g/m2(ii) a The needling depth is 6-25 mm, and the needling density is 4 times/cm28 times/cm2Injection density of 1 times/cm22 times/cm2(ii) a The number ratio of the injection needles to the acupuncture needles is 1: 4-6, wherein the length of the injection needle is longer than that of the acupuncture needle by 2 +/-0.1 mm.
8. The preparation method of the carbon-ceramic composite material heater as claimed in claim 1, wherein in the step ⑵, the pressure during injection is 0.25MPa to 0.45MPa, and the injection amount of the ceramic slurry is 2.0 g/cm3～4.67g/㎝3The introduction amount of the ceramic powder in the carbon-ceramic composite material heater wet blank is 0.2 g/cm3～1.4 g/㎝3。
9. The method as claimed in claim 1, wherein in the step ⑸, the natural gas or methane or propane is used as raw material, the deposition pressure is 1 kPa-3 kPa, and the deposition temperature is 950 ℃ -1200 ℃ during the vapor deposition.
10. A carbon-ceramic composite material heater prepared by the method as claimed in claim 3, 4, 5, 6, 7, 8 or 9, and characterized in that the heater has an open porosity of 1-9% and a density of 1.5g/cm3～2.3g/㎝3The bending strength is 250 MPa-480 MPa, and the resistivity is 10 mu omega-300 mu omega-m.
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